反応 #82076

反応方程式

3-chloro-2,4-difluoro-6-nitroaniline

SnCl2

→

solid

収率 95.6%

4-Chloro-3,5-difluoro-1,2-phenylenediamine

収率 95.6%

溶媒

ethanol

反応条件

後処理

1. 1
   その他The solution was evaporated
2. 2
   その他to remove the ethanol
3. 3
   workup.ADDITIONThe residue was treated with 2N NaOH to pH=13
4. 4
   抽出The mixture was extracted by CHCl3 (3×10 mL)
5. 5
   乾燥The extract was dried (MgSO4)
6. 6
   その他evaporated

実験手順

A solution of 348 mg (1.67 mmol) of 3-chloro-2,4-difluoro-6-nitroaniline and 1.57 g (8.28 mmol) of SnCl2 in 8 mL of ethanol was heated at 70° C. for 2 h. The solution was evaporated to remove the ethanol. The residue was treated with 2N NaOH to pH=13. White precipitate was observed. The mixture was extracted by CHCl3 (3×10 mL). The extract was dried (MgSO4) and evaporated to leave a red solid (285 mg, 95%), mp 77°-78° C. 1H NMR (CDCl3), 3.156 (b, 2), 3.704 (b, 2), 6.352 (dd, 1, J=1.86, 9.95).

出典